CN104280354A - Method for detecting sulfur content of coal test sample - Google Patents
Method for detecting sulfur content of coal test sample Download PDFInfo
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- CN104280354A CN104280354A CN201410582065.1A CN201410582065A CN104280354A CN 104280354 A CN104280354 A CN 104280354A CN 201410582065 A CN201410582065 A CN 201410582065A CN 104280354 A CN104280354 A CN 104280354A
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Abstract
The invention discloses a method for detecting the sulfur content of a coal test sample. The method comprises the steps of firstly igniting the coal test sample in an electric arc ignition furnace under the condition of oxygen to generate burner gas, detecting an optical parameter of gas absorption liquid, then feeding the burner gas subjected to filtration and volume measurement into the gas absorption liquid, performing ultrasonic vibration on the gas absorption liquid by an ultrasonic vibration device, titrating a potassium iodide solution into the gas absorption solution, adjusting the titration speed according to the color change of the gas absorption liquid, ending the titration when the optical parameter of the gas absorption liquid returns to an initial value, and obtaining the full sulfur content of the sample according to the amount of the titrating potassium iodide solution and the gas volume measured by a flowmeter. According to the method for detecting the sulfur content of the coal test sample, the full sulfur content of the test sample can be quickly and efficiently detected; by ultrasonic vibration in a gas absorption process, dissolving of sulfur dioxide is accelerated, and the detection precision of the optical parameter of the gas absorption liquid is improved.
Description
Technical field
The present invention relates to material analysis techniques field, particularly relate to a kind of coal sample sulfur content detection method.
Background technology
In coal, iron and steel and various exploitation of mineral resources field, need that component concentration is carried out to sample and carry out determination and analysis, especially the sulfur content in sample, it is one of important indicator of the quality of evaluating material, simultaneously contained in these materials sulphur produces sulfurous gas through burning, one of its principal ingredient being atmospheric pollution, therefore, the analysis of the total sulphur content in material is in widespread attention.
Usually, adopt the total sulphur content in constant sulphur appliance detection coal, iron and steel and various mineral products, constant sulphur appliance utilizes Coulomb equation, pass into electrolytic cell by gas sample burning produced, the potential change between detecting electrode determines the total sulphur content in sample, but, potential change influence factor in electrolytic cell is more, after electrolytic solution simultaneously in electrolytic cell and electrode generation Electrolysis, be easily corroded pollution, so that greatly affect the accuracy of detection of constant sulphur appliance.
Summary of the invention
For solving the technical matters existed in background technology, the present invention proposes a kind of coal sample sulfur content detection method, and rapidly and efficiently can detect total sulphur content contained in coal sample, error is little, accuracy of detection is high.
A kind of coal sample sulfur content detection method that the present invention proposes, comprises the following steps: burning test specimen, filters furnace gas, measurement volumes, gas absorption, the titration of iodine potassium, result of calculation;
Burning test specimen: sample is put into arc ignition stove, under Oxygen Condition, arc ignition coal sample produces furnace gas;
Filter furnace gas: filter solid dust contained in furnace gas;
Measurement volumes: adopt the filtered furnace gas volume of flowmeter survey;
Gas absorption: adopt fiber laser arrays device to detect the initial optical parameter c1 of gas absorption liquid, furnace gas after filtering is passed in gas absorption liquid, adopt ultrasonic vibration installation to carry out ultrasonic vibration to gas absorption liquid simultaneously, wherein gas absorption liquid is the starch solution being added with iodine potassium solution in advance, and is acid by the pH value of adding hydrochloric acid conditioning solution;
Iodine potassium titration: when the color of gas absorption liquid starts to fade, rapid titration iodine potassium solution in gas absorption liquid, when starch solution slowly fades, reduce rate of titration, close ultrasonic vibration installation simultaneously, adopt optical fiber detector again to detect the optical parametric c2 of gas absorption liquid, as c2=c1, titration terminates;
Result of calculation: the amount calculating the sulphuric dioxide absorbed in gas absorption liquid according to the gauge of the iodine potassium solution of titration, thus according to the gas volume of flowmeter survey and the total sulphur content measured in sample of sulphuric dioxide that wherein contains.
Preferably, in gas absorption process, gas absorption liquid adopts the starch solution of 0.8g/L, and its pH value is 3-5.
Preferably, after the titration of iodine potassium terminates, again ultrasonic vibration is carried out to gas absorption liquid.
In the present invention, the coal sample sulfur content detection method proposed, the step comprised has: burning test specimen, filter furnace gas, measurement volumes, gas absorption, the titration of iodine potassium, result of calculation, first the coal sample that ignites under Oxygen Condition in arc ignition stove produces furnace gas, detect the optical parametric of gas absorption liquid, then will pass in gas absorption liquid with the furnace gas of measurement volumes after filtration, adopt ultrasonic vibration installation to carry out ultrasonic vibration to gas absorption liquid simultaneously, titration iodine potassium solution in gas absorption liquid, and regulate rate of titration according to the color change of gas absorption liquid, when the optical parametric of gas absorption liquid gets back to initial value, titration terminates, the total sulphur content in sample is obtained according to the amount of iodine potassium solution of titration and the gas volume of flowmeter survey.By the coal sample sulfur content detection method of above-mentioned optimal design, the total sulphur content that can rapidly and efficiently contain in test samples, carry out the dissolving that ultrasonic vibration accelerates sulphuric dioxide in gas absorption process, and improve the accuracy of detection of the optical parametric of gas absorption liquid.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of coal sample sulfur content detection method that the present invention proposes.
Embodiment
As shown in Figure 1, Fig. 1 is the structural representation of a kind of coal sample sulfur content detection method that the present invention proposes.
With reference to Fig. 1, the coal sample sulfur content detection method that the present invention proposes, comprises the following steps: burning test specimen, filters furnace gas, measurement volumes, gas absorption, the titration of iodine potassium, result of calculation;
Burning test specimen: sample is put into arc ignition stove, under Oxygen Condition, arc ignition coal sample produces furnace gas;
Filter furnace gas: filter solid dust contained in furnace gas;
Measurement volumes: adopt the filtered furnace gas volume of flowmeter survey;
Gas absorption: adopt fiber laser arrays device to detect the initial optical parameter c1 of gas absorption liquid, furnace gas after filtering is passed in gas absorption liquid, adopt ultrasonic vibration installation to carry out ultrasonic vibration to gas absorption liquid simultaneously, wherein gas absorption liquid is the starch solution of the 0.8g/L being added with iodine potassium solution in advance, and is 3-5 by the pH value of adding hydrochloric acid conditioning solution;
Iodine potassium titration: when the color of gas absorption liquid starts to fade, rapid titration iodine potassium solution in gas absorption liquid, when starch solution slowly fades, reduce rate of titration, close ultrasonic vibration installation simultaneously, adopt optical fiber detector again to detect the optical parametric c2 of gas absorption liquid, as c2=c1, titration terminates;
Result of calculation: the amount calculating the sulphuric dioxide absorbed in gas absorption liquid according to the gauge of the iodine potassium solution of titration, thus according to the gas volume of flowmeter survey and the total sulphur content measured in sample of sulphuric dioxide that wherein contains.
In the present embodiment, the coal sample sulfur content detection method proposed, the step comprised has: burning test specimen, filter furnace gas, measurement volumes, gas absorption, the titration of iodine potassium, result of calculation, first the coal sample that ignites under Oxygen Condition in arc ignition stove produces furnace gas, detect the optical parametric of gas absorption liquid, then will pass in gas absorption liquid with the furnace gas of measurement volumes after filtration, adopt ultrasonic vibration installation to carry out ultrasonic vibration to gas absorption liquid simultaneously, titration iodine potassium solution in gas absorption liquid, and regulate rate of titration according to the color change of gas absorption liquid, when the optical parametric of gas absorption liquid gets back to initial value, titration terminates, the total sulphur content in sample is obtained according to the amount of iodine potassium solution of titration and the gas volume of flowmeter survey.By the coal sample sulfur content detection method of above-mentioned optimal design, the total sulphur content that can rapidly and efficiently contain in test samples, carry out the dissolving that ultrasonic vibration accelerates sulphuric dioxide in gas absorption process, and improve the accuracy of detection of the optical parametric of gas absorption liquid.
The method detecting sulfur content in coal sample is described in detail in an embodiment below in conjunction with coal sample sulfur content detecting instrument.
The coal sample sulfur content detecting instrument that the present embodiment proposes, comprising: arc ignition stove, draft tube, gas absorption bottle, ultrasonic vibration installation, incident optical, detection fiber, starch liquid storage bottle, feed tube, iodine potassium liquid storage bottle, connecting pipe and buret;
Gas absorption bottle adopts light screening material to make, which is provided with openable view window, gas absorption bottle is also provided with gas access, gas vent, the first inlet, the second inlet, waste liquid outlet, light entrance port and optical emission exit, gas outlet is connected with gas outlet, and light entrance port and optical emission exit are oppositely arranged;
Draft tube one end is sealedly connected on the gas access place of gas absorption bottle, and the other end seals with arc ignition stove and is communicated with, and draft tube is provided with flowmeter and filtrator, and filtrator is for filtering solid impurity contained in furnace gas;
Feed tube one end is sealedly connected on the first inlet place of gas absorption bottle, and the other end seals with starch liquid storage bottle and is communicated with, and feed tube is provided with the first operation valve;
Buret is positioned at above gas detect bottle, and its one end is connected to the second inlet place of gas absorption bottle, and the other end is connected with iodine potassium liquid storage bottle by connecting pipe, and buret is provided with the second operation valve, and connecting pipe is provided with the 3rd operation valve;
Incident optical and detection fiber are oppositely arranged, and the output terminal of incident optical is connected to the light entrance port place of gas absorption bottle, and the input end of detection fiber is connected to optical emission exit place;
Ultrasonic vibration installation is for making the solution ultrasonic vibration in gas absorption bottle.
In the process of the total sulphur content of the coal sample sulfur content detection method test samples of the present embodiment, detected sample is placed in arc ignition stove, first feeding device is to the starch solution of the 0.8g/L of pre-add in gas absorption bottle, iodine potassium liquid storage bottle via connecting pipe to pre-add iodine potassium solution in buret, the color of starch solution is made to become blueness, by adding hydrochloric acid, the pH value of the solution in gas absorption bottle is adjusted to 3-5, incident optical and detection fiber detect the initial optical parameter of solution in gas absorption bottle, then pass into oxygen in arc ignition stove and arc ignition is carried out to coal sample, the furnace gas produced enters draft tube, enter in the solution in gas absorption bottle after filtrator inner filtration solid impurity, ultrasonic vibration installation makes the solution ultrasonic vibration in gas absorption bottle simultaneously, accelerate gas absorption in the solution, then the color change that solution observed by view window is opened, when the color of solution starts to fade, buret is to rapid titration iodine potassium solution in gas absorption bottle, when solution slowly fades, close view window, slow titration iodine potassium solution, when detection fiber detects that the optical parametric of solution is got back to initial value and no longer changes, titration terminates, by accurately monitoring the optical parametric change of gas absorption liquid, carry out the iodine potassium solution of accurate titration, the amount of the sulphuric dioxide absorbed in gas absorption liquid can be drawn, thus the total sulphur content obtained in burning test specimen, after detection terminates, the unabsorbed gas from gas outlet of starch solution is discharged, and reacted solution is discharged from waste liquid port.
In a specific embodiment, after the titration of iodine potassium terminates, again ultrasonic vibration is carried out to gas absorption liquid, in order to avoid the starch in gas absorption liquid is attached on the bottle wall of gas absorption bottle, be convenient to the cleaning of gas absorption bottle, improve the degree of accuracy of testing result further.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (3)
1. a coal sample sulfur content detection method, is characterized in that, comprises the following steps: burning test specimen, filters furnace gas, measurement volumes, gas absorption, the titration of iodine potassium, result of calculation;
Burning test specimen: sample is put into arc ignition stove, under Oxygen Condition, arc ignition coal sample produces furnace gas;
Filter furnace gas: filter solid dust contained in furnace gas;
Measurement volumes: adopt the filtered furnace gas volume of flowmeter survey;
Gas absorption: adopt fiber laser arrays device to detect the initial optical parameter c1 of gas absorption liquid, furnace gas after filtering is passed in gas absorption liquid, adopt ultrasonic vibration installation to carry out ultrasonic vibration to gas absorption liquid simultaneously, wherein gas absorption liquid is the starch solution being added with iodine potassium solution in advance, and is acid by the pH value of adding hydrochloric acid conditioning solution;
Iodine potassium titration: when the color of gas absorption liquid starts to fade, rapid titration iodine potassium solution in gas absorption liquid, when starch solution slowly fades, reduce rate of titration, close ultrasonic vibration installation simultaneously, adopt optical fiber detector again to detect the optical parametric c2 of gas absorption liquid, as c2=c1, titration terminates;
Result of calculation: the amount calculating the sulphuric dioxide absorbed in gas absorption liquid according to the gauge of the iodine potassium solution of titration, thus according to the gas volume of flowmeter survey and the total sulphur content measured in sample of sulphuric dioxide that wherein contains.
2. coal sample sulfur content detection method according to claim 1, is characterized in that, in gas absorption process, gas absorption liquid adopts the starch solution of 0.8g/L, and its pH value is 3-5.
3. coal sample sulfur content detection method according to claim 1, is characterized in that, after the titration of iodine potassium terminates, again carry out ultrasonic vibration to gas absorption liquid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106855473A (en) * | 2016-12-01 | 2017-06-16 | 清华大学 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
| CN107643287A (en) * | 2017-11-13 | 2018-01-30 | 中钢集团马鞍山矿山研究院有限公司 | A kind of constant sulphur appliance of automatic Titration |
| CN114289451A (en) * | 2021-12-27 | 2022-04-08 | 鹤庆北衙矿业有限公司 | Ultrasonic synergetic SO2Method for degrading gold cyanidation tailings |
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| CN2591624Y (en) * | 2002-01-30 | 2003-12-10 | 李志标 | Automatic analysis meter for cement, carbon & sulfur |
| CN2819221Y (en) * | 2005-09-08 | 2006-09-20 | 孙笑欢 | Determined part of automatic carbon sulfur analyzer |
| CN102323264A (en) * | 2011-09-30 | 2012-01-18 | 中国冶金矿业鞍山冶金设计研究院有限责任公司 | Method and device for testing content of sulfur in iron ore |
| CN102818876A (en) * | 2012-08-23 | 2012-12-12 | 芜湖新兴铸管有限责任公司 | Method for determining sulfur content in iron ore by combustion iodometry |
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2014
- 2014-10-27 CN CN201410582065.1A patent/CN104280354A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2591624Y (en) * | 2002-01-30 | 2003-12-10 | 李志标 | Automatic analysis meter for cement, carbon & sulfur |
| CN2819221Y (en) * | 2005-09-08 | 2006-09-20 | 孙笑欢 | Determined part of automatic carbon sulfur analyzer |
| CN102323264A (en) * | 2011-09-30 | 2012-01-18 | 中国冶金矿业鞍山冶金设计研究院有限责任公司 | Method and device for testing content of sulfur in iron ore |
| CN102818876A (en) * | 2012-08-23 | 2012-12-12 | 芜湖新兴铸管有限责任公司 | Method for determining sulfur content in iron ore by combustion iodometry |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106855473A (en) * | 2016-12-01 | 2017-06-16 | 清华大学 | A kind of method for preparing the fluid sample of carbon 14 in live graphite |
| CN107643287A (en) * | 2017-11-13 | 2018-01-30 | 中钢集团马鞍山矿山研究院有限公司 | A kind of constant sulphur appliance of automatic Titration |
| CN114289451A (en) * | 2021-12-27 | 2022-04-08 | 鹤庆北衙矿业有限公司 | Ultrasonic synergetic SO2Method for degrading gold cyanidation tailings |
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Effective date of registration: 20151126 Address after: The economic development zone of Longgang road and Yaohai road junction Qi Garden real District of Hefei City, Anhui province 230000 two B group 39 building 803 room Applicant after: HEFEI ZAIDE MACROMOLECULE MATERIAL CO., LTD. Address before: 230000 No. 45 West Chaohu Road, upper town, Feixi County, Anhui, Hefei Applicant before: HEFEI ZHUOYUE ANALYTICAL INSTRUMENTS CO., LTD. |
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Application publication date: 20150114 |